液-液分散微萃取-高效液相色谱法测定豆制品中的碱性嫩黄O.docVIP

  离子液体/液-液分散微萃取-高效液相色谱 法测定豆制品中的碱性嫩黄 O# 李晶1,2，徐济仓1，李雪梅1** 5 10 15 20 25 30 35 （1. 云南烟草科学研究院，昆明 650106； 2. 浙江大学智能系统与控制研究所，工业控制技术国家重点实验室，杭州 310058） 摘要：建立了基于离子液体液-液分散微萃取与高效液相色谱光电二极管阵列检测法 （HPLC-DAD）检测豆制品中的碱性嫩黄 O 的新方法。该方法将萃取和富集一步完成，对于影 响萃取富集效率的因素进行优化：例如萃取离子液体的种类、 萃取离子液体的体积、分散 溶剂的种类、分散溶剂的体积、pH 影响和盐效应等。在优化的条件下，碱性嫩黄 O 在 5 μ g/L-5000μg/L 浓度范围内存在良好的线性关系，线性相关系数 r=0.9998;检出限为 2.2μ g/L（S/N=3）。该方法能较好的应用于豆制品中碱性嫩黄 O 的检测，在不同的加标水平下， 平均回收率在 98.2%，RSD6.8%(n=5)。本方法具有操作简单、成本较低、溶剂消耗低、灵 敏度高和干扰较小等特点，可以应用于豆制品中痕量碱性嫩黄 O 的检测。 关键词：离子液体；液-液分散微萃取；高效液相色谱法；碱性嫩黄 O；富集 中图分类号：O657.7+2 Determination of auramine O by ionic liquid dispersive liquid-liquid microextraction in soya bean products samples Li Jing1,2, Xu Jicang1, Li Xuemei1 (1. Yunnan Academy of Tobacco Science , KunMing 650106; 2. State Key Laboratory of Industrial Control Technology, Institute of Cyber-Systems and Control, Zhejiang University, HangZhou 310058) Abstract: A novel microextraction method termed ionic dispersive liquid-liquid microextraction (IL-DLLME) combining high-performance liquid chromatography with diode array detection (HPLC-DAD) was developed for the determination of auramine O in soya bean products samples. This technique combines extraction and concentration of the analytes into one step, and the ionic liquid was used instead of a volatile organic solvent as the extraction solvent. Several important parameters influencing the extraction and concentration efficiency such as the type and volume of extraction solvent, the type and volume of disperser solvent, the value of pH as well as the salt effects were further investigated. Under the optimized conditions, linearity of the method was observed for auramine O in the range from 5 μg/L to 5000μg/L with the accepted correlation coefficient (r0.9990). The limit of detection (S/N=3) was 2.2μg/L. The average recovery of auramine O spiked in soy bean product samples at different spiked levels was 98.2% with the relative standard deviation (RSD6.8%, n=5). With the advantages